Use of solid-phase microextraction followed by on-column silylation for determining chlorinated bisphenol A in human plasma by gas chromatography-mass spectrometry

被引:41
作者
del Olmo, M [1 ]
Zafra, A [1 ]
Suárez, B [1 ]
Gonzalez-Casado, A [1 ]
Taoufiki, J [1 ]
Vílchez, JL [1 ]
机构
[1] Univ Granada, Dept Analyt Chem, E-18071 Granada, Spain
来源
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES | 2005年 / 817卷 / 02期
关键词
chlorinated bisphenol A; solid-phase microextraction; column silylation; GC-MS; human plasma;
D O I
10.1016/j.jchromb.2004.11.059
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
In this study, a solid-phase microextraction (SPME) method based on poly(acrylate)-coated fibres has been developed for detection and quantification of chlorinated bisphenol A in human plasma due to the need for an assessment of human exposure to them. After desorption of the analytes for 7 min at 300 degreesC, they were directly derivatized in the GC injector port by injection of 2 muL of diluted bis(trimethylsilyl)trifluoroacetamide (BSTFA). The formation of trimethylsilylate derivatives improves the selectivity, sensitivity and performance of the chromatographic properties obtained when the analytes are directly separated. Quantification was carried out using single-ion monitoring (SIM). The respective chloroderivative molecular ions appear at 406, 440, 474 and 508 m/z; whereas the base peaks corresponding to a loss of a methyl group in all cases appear at 391, 425,459 and 493 m/z for mono-, di-, tri- and tetrabisphenol A, respectively. Deuterated bisphenol A (BPA-d(16)) was used as an internal standard. The method was applied to the determination of Cl-BPA, Cl-2-BPA, Cl-3-BPA and Cl-4-BPA at very low concentration levels in plasma. Recovery efficiencies were close to 100% in all cases. (C) 2004 Elsevier B.V. All rights reserved.
引用
收藏
页码:167 / 172
页数:6
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